#------------------------------------------------------------------------------ #$Date: 2021-11-06 22:32:09 +0200 (Sat, 06 Nov 2021) $ #$Revision: 270486 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/09/7060957.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7060957 loop_ _publ_author_name 'Kotov, Vitalii Yu.' 'Buikin, Pert A.' 'Ilyukhin, Andrey B.' 'Korlyukov, Alexander A.' 'Dorovatovskii, Pavel V.' _publ_section_title ; Synthesis and first-principles study of structural, electronic and optical properties of tetragonal hybrid halobismuthathes [Py2(XK)]2[Bi2Br10−xIx] ; _journal_issue 39 _journal_name_full 'New Journal of Chemistry' _journal_page_first 18349 _journal_page_last 18357 _journal_paper_doi 10.1039/D1NJ02390J _journal_volume 45 _journal_year 2021 _chemical_absolute_configuration unk _chemical_formula_moiety 'C18 H18 N2, Bi Br5' _chemical_formula_sum 'C18 H18 Bi Br5 N2' _chemical_formula_weight 870.87 _space_group_IT_number 79 _space_group_name_Hall 'I 4' _space_group_name_H-M_alt 'I 4' _symmetry_cell_setting tetragonal _symmetry_Int_Tables_number 79 _symmetry_space_group_name_Hall 'I 4' _symmetry_space_group_name_H-M 'I 4' _atom_sites_solution_hydrogens geom _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4.3 _audit_creation_date 2018-11-19T22:52:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_update_record ; 2021-02-22 deposited with the CCDC. 2021-08-31 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.890(2) _cell_length_b 12.890(2) _cell_length_c 13.861(2) _cell_measurement_reflns_used 5313 _cell_measurement_temperature 120(2) _cell_measurement_theta_max 32.89 _cell_measurement_theta_min 2.23 _cell_volume 2303.0(6) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/1 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-2018 (Sheldrick, 2015)' _diffrn_ambient_temperature 120(2) _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_unetI/netI 0.0395 _diffrn_reflns_Laue_measured_fraction_full 1 _diffrn_reflns_Laue_measured_fraction_max 1 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 16399 _diffrn_reflns_point_group_measured_fraction_full 1 _diffrn_reflns_point_group_measured_fraction_max 1 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.497 _diffrn_reflns_theta_min 2.158 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 16.336 _exptl_absorpt_correction_T_max 0.0551 _exptl_absorpt_correction_T_min 0.0123 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS 2014/5' _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 2.512 _exptl_crystal_description block _exptl_crystal_F_000 1592 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 2.487 _refine_diff_density_min -1.088 _refine_diff_density_rms 0.162 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.466(9) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 122 _refine_ls_number_reflns 3837 _refine_ls_number_restraints 1 _refine_ls_restrained_S_all 1.053 _refine_ls_R_factor_all 0.0313 _refine_ls_R_factor_gt 0.0276 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0300P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.0657 _reflns_Friedel_coverage 0.93 _reflns_Friedel_fraction_full 1 _reflns_Friedel_fraction_max 1 _reflns_number_gt 3570 _reflns_number_total 3837 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj02390j2.cif _cod_data_source_block 1 _cod_depositor_comments 'Adding full bibliography for 7060957--7060960.cif.' _cod_original_cell_volume 2303.0(8) _cod_database_code 7060957 _shelx_res_file ; TITL 1 in I4 shelx.res created by SHELXL-2018/1 at 22:52:16 on 19-Nov-2018 CELL 0.71073 12.890 12.890 13.861 90.000 90.000 90.000 ZERR 4 0.002 0.002 0.002 0.000 0.000 0.000 LATT -2 SYMM -X, -Y, Z SYMM -Y, X, Z SYMM Y, -X, Z SFAC C H N BR BI UNIT 72 72 8 20 4 TEMP -153.000 SHEL 10 .68 ACTA L.S. 4 BOND $H htab EQIV $3 y, -x+1, z HTAB C1 Br1_$3 EQIV $5 -y+3/2, x+1/2, z+1/2 HTAB C2 Br3_$5 HTAB C4 Br1_$5 EQIV $6 y, -x+1, z+1 HTAB C5 Br3_$6 HTAB C6 Br3_$6 HTAB C6 Br1_$3 twin WGHT 0.030000 BASF 0.46583 FVAR 0.12273 BI1 5 0.500000 0.500000 0.322158 10.25000 0.01722 0.01722 = 0.02751 0.00000 0.00000 0.00000 BI2 5 0.500000 0.500000 -0.122547 10.25000 0.02005 0.02005 = 0.02942 0.00000 0.00000 0.00000 BR1 4 0.282468 0.464296 0.320197 11.00000 0.01898 0.02125 = 0.02736 -0.00170 0.00009 -0.00059 BR2 4 0.500000 0.500000 0.517072 10.25000 0.02334 0.02334 = 0.02808 0.00000 0.00000 0.00000 BR3 4 0.284770 0.463686 -0.150122 11.00000 0.02305 0.02331 = 0.03201 0.00131 -0.00505 -0.00094 BR4 4 0.500000 0.500000 0.071652 10.25000 0.03919 0.03919 = 0.03446 0.00000 0.00000 0.00000 N1 3 0.647910 0.754265 0.585721 11.00000 0.02336 0.01572 = 0.01963 -0.00126 -0.00008 0.00072 C1 1 0.696217 0.745926 0.500352 11.00000 0.02263 0.03143 = 0.01647 0.00225 0.00284 0.00508 AFIX 43 H1A 2 0.657795 0.747280 0.441878 11.00000 -1.20000 AFIX 0 C2 1 0.805674 0.735054 0.498981 11.00000 0.02376 0.03022 = 0.03331 0.00843 0.00823 0.00753 AFIX 43 H2A 2 0.841438 0.729459 0.439280 11.00000 -1.20000 AFIX 0 C3 1 0.859607 0.732653 0.584037 11.00000 0.02174 0.02042 = 0.04514 -0.00075 -0.00248 0.00286 AFIX 43 H3A 2 0.933125 0.727481 0.583772 11.00000 -1.20000 AFIX 0 C4 1 0.805521 0.737878 0.671180 11.00000 0.02991 0.03641 = 0.03108 -0.00689 -0.01059 0.00438 AFIX 43 H4A 2 0.841500 0.734022 0.730888 11.00000 -1.20000 AFIX 0 C5 1 0.700055 0.748622 0.669314 11.00000 0.03486 0.03054 = 0.02210 -0.00529 0.00129 0.00602 AFIX 43 H5A 2 0.662915 0.752166 0.728422 11.00000 -1.20000 AFIX 0 C6 1 0.534855 0.776711 0.586206 11.00000 0.01924 0.01633 = 0.02887 -0.00100 0.00019 0.00118 AFIX 23 H6A 2 0.502558 0.745644 0.644211 11.00000 -1.20000 H6B 2 0.501977 0.745606 0.528502 11.00000 -1.20000 AFIX 0 C7 1 0.517356 0.893427 0.586249 11.00000 0.01755 0.01764 = 0.02164 -0.00096 0.00032 -0.00087 C8 1 0.508602 0.945940 0.499209 11.00000 0.02508 0.01928 = 0.01759 -0.00169 0.00268 0.00194 AFIX 43 H8A 2 0.514165 0.909302 0.439966 11.00000 -1.20000 AFIX 0 C9 1 0.508692 0.946312 0.672660 11.00000 0.02543 0.01956 = 0.02012 0.00181 -0.00025 -0.00094 AFIX 43 H9A 2 0.514515 0.909910 0.732008 11.00000 -1.20000 AFIX 0 HKLF 4 REM 1 in I4 REM R1 = 0.0276 for 3570 Fo > 4sig(Fo) and 0.0313 for all 3837 data REM 122 parameters refined using 1 restraints END WGHT 0.0266 0.4933 REM Instructions for potential hydrogen bonds HTAB C1 Br1_$3 HTAB C2 Br3_$5 HTAB C4 Br1_$5 HTAB C5 Br3_$6 HTAB C6 Br3_$6 HTAB C6 Br1_$3 REM Highest difference peak 2.487, deepest hole -1.088, 1-sigma level 0.162 Q1 1 0.5000 0.5000 -0.1791 10.25000 0.05 2.49 Q2 1 0.5000 0.5000 0.2625 10.25000 0.05 2.37 Q3 1 0.5000 0.5000 -0.0570 10.25000 0.05 1.74 Q4 1 0.5000 0.5000 0.3789 10.25000 0.05 1.67 Q5 1 0.5000 0.5000 0.1253 10.25000 0.05 1.40 Q6 1 0.5222 0.5530 0.3200 11.00000 0.05 1.07 Q7 1 0.5196 0.5562 -0.1292 11.00000 0.05 0.89 Q8 1 0.5000 0.5000 -0.0033 10.25000 0.05 0.85 Q9 1 0.5000 0.5000 0.5724 10.25000 0.05 0.84 Q10 1 0.5000 0.5000 0.6458 10.25000 0.05 0.75 Q11 1 0.5000 0.5000 0.2021 10.25000 0.05 0.70 Q12 1 0.3780 0.5348 -0.1244 11.00000 0.05 0.60 Q13 1 0.5437 0.6163 0.3168 11.00000 0.05 0.51 Q14 1 0.3758 0.3796 -0.2195 11.00000 0.05 0.49 Q15 1 0.6438 0.6199 0.6052 11.00000 0.05 0.48 Q16 1 0.6614 0.6396 0.7361 11.00000 0.05 0.48 Q17 1 0.3374 0.4405 0.3186 11.00000 0.05 0.47 Q18 1 0.8851 0.8645 0.6807 11.00000 0.05 0.45 Q19 1 0.6407 0.6393 0.7975 11.00000 0.05 0.45 Q20 1 0.8806 0.8653 0.5158 11.00000 0.05 0.45 ; _shelx_res_checksum 93038 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Bi1 Bi 0.5 0.5 0.32216(3) 0.02065(11) Uani 1 4 d S T P . . Bi2 Bi 0.5 0.5 -0.12255(3) 0.02317(13) Uani 1 4 d S T P . . Br1 Br 0.28247(5) 0.46430(5) 0.32020(5) 0.02253(13) Uani 1 1 d . . . . . Br2 Br 0.5 0.5 0.51707(11) 0.0249(3) Uani 1 4 d S T P . . Br3 Br 0.28477(6) 0.46369(6) -0.15012(5) 0.02612(17) Uani 1 1 d . . . . . Br4 Br 0.5 0.5 0.07165(12) 0.0376(4) Uani 1 4 d S T P . . N1 N 0.6479(4) 0.7543(3) 0.5857(4) 0.0196(10) Uani 1 1 d . . . . . C1 C 0.6962(7) 0.7459(6) 0.5004(4) 0.0235(16) Uani 1 1 d . . . . . H1A H 0.657795 0.74728 0.441878 0.028 Uiso 1 1 calc R U . . . C2 C 0.8057(7) 0.7351(7) 0.4990(5) 0.0291(18) Uani 1 1 d . . . . . H2A H 0.841438 0.729459 0.43928 0.035 Uiso 1 1 calc R U . . . C3 C 0.8596(5) 0.7327(5) 0.5840(6) 0.0291(15) Uani 1 1 d . . . . . H3A H 0.933125 0.727481 0.583772 0.035 Uiso 1 1 calc R U . . . C4 C 0.8055(7) 0.7379(7) 0.6712(6) 0.0325(19) Uani 1 1 d . . . . . H4A H 0.8415 0.734022 0.730888 0.039 Uiso 1 1 calc R U . . . C5 C 0.7001(7) 0.7486(6) 0.6693(5) 0.0292(17) Uani 1 1 d . . . . . H5A H 0.662915 0.752166 0.728422 0.035 Uiso 1 1 calc R U . . . C6 C 0.5349(4) 0.7767(4) 0.5862(6) 0.0215(11) Uani 1 1 d . . . . . H6A H 0.502558 0.745644 0.644211 0.026 Uiso 1 1 calc R U . . . H6B H 0.501977 0.745606 0.528502 0.026 Uiso 1 1 calc R U . . . C7 C 0.5174(4) 0.8934(4) 0.5862(5) 0.0189(10) Uani 1 1 d . . . . . C8 C 0.5086(6) 0.9459(6) 0.4992(4) 0.0206(14) Uani 1 1 d . . . . . H8A H 0.514165 0.909302 0.439966 0.025 Uiso 1 1 calc R U . . . C9 C 0.5087(5) 0.9463(6) 0.6727(4) 0.0217(14) Uani 1 1 d . . . . . H9A H 0.514515 0.90991 0.732008 0.026 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Bi1 0.01722(16) 0.01722(16) 0.0275(2) 0 0 0 Bi2 0.02005(19) 0.02005(19) 0.0294(2) 0 0 0 Br1 0.0190(3) 0.0212(3) 0.0274(3) -0.0017(3) 0.0001(3) -0.0006(2) Br2 0.0233(4) 0.0233(4) 0.0281(6) 0 0 0 Br3 0.0231(4) 0.0233(4) 0.0320(3) 0.0013(2) -0.0050(2) -0.0009(3) Br4 0.0392(5) 0.0392(5) 0.0345(8) 0 0 0 N1 0.023(2) 0.0157(19) 0.020(3) -0.0013(18) 0.000(2) 0.0007(16) C1 0.023(4) 0.031(4) 0.016(3) 0.002(2) 0.003(2) 0.005(3) C2 0.024(4) 0.030(4) 0.033(4) 0.008(3) 0.008(3) 0.008(3) C3 0.022(3) 0.020(3) 0.045(5) -0.001(3) -0.002(3) 0.003(2) C4 0.030(4) 0.036(5) 0.031(4) -0.007(3) -0.011(3) 0.004(3) C5 0.035(4) 0.031(4) 0.022(3) -0.005(2) 0.001(3) 0.006(3) C6 0.019(2) 0.016(2) 0.029(4) -0.001(2) 0.000(2) 0.0012(18) C7 0.018(2) 0.018(2) 0.022(3) -0.001(2) 0.000(2) -0.0009(17) C8 0.025(4) 0.019(4) 0.018(3) -0.0017(19) 0.003(2) 0.002(3) C9 0.025(3) 0.020(3) 0.020(3) 0.002(2) 0.000(2) -0.001(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Bi Bi -4.1077 10.2566 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Br2 Bi1 Br1 90.548(17) . 2_665 ? Br2 Bi1 Br1 90.548(16) . 3_655 ? Br1 Bi1 Br1 90 2_665 3_655 ? Br2 Bi1 Br1 90.548(16) . . ? Br1 Bi1 Br1 178.90(3) 2_665 . ? Br1 Bi1 Br1 90 3_655 . ? Br2 Bi1 Br1 90.548(16) . 4_565 ? Br1 Bi1 Br1 90 2_665 4_565 ? Br1 Bi1 Br1 178.90(3) 3_655 4_565 ? Br1 Bi1 Br1 90 . 4_565 ? Br4 Bi2 Br3 97.736(18) . . ? Br4 Bi2 Br3 97.737(18) . 3_655 ? Br3 Bi2 Br3 88.962(5) . 3_655 ? Br4 Bi2 Br3 97.737(18) . 2_665 ? Br3 Bi2 Br3 164.53(4) . 2_665 ? Br3 Bi2 Br3 88.962(5) 3_655 2_665 ? Br4 Bi2 Br3 97.737(18) . 4_565 ? Br3 Bi2 Br3 88.961(5) . 4_565 ? Br3 Bi2 Br3 164.53(4) 3_655 4_565 ? Br3 Bi2 Br3 88.962(5) 2_665 4_565 ? C1 N1 C5 121.7(5) . . ? C1 N1 C6 118.4(6) . . ? C5 N1 C6 119.9(6) . . ? N1 C1 C2 118.8(7) . . ? N1 C1 H1A 120.6 . . ? C2 C1 H1A 120.6 . . ? C3 C2 C1 119.7(7) . . ? C3 C2 H2A 120.1 . . ? C1 C2 H2A 120.1 . . ? C2 C3 C4 119.4(6) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 119.0(7) . . ? C5 C4 H4A 120.5 . . ? C3 C4 H4A 120.5 . . ? N1 C5 C4 121.3(7) . . ? N1 C5 H5A 119.3 . . ? C4 C5 H5A 119.3 . . ? N1 C6 C7 109.8(4) . . ? N1 C6 H6A 109.7 . . ? C7 C6 H6A 109.7 . . ? N1 C6 H6B 109.7 . . ? C7 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C9 C7 C8 120.4(5) . . ? C9 C7 C6 120.0(6) . . ? C8 C7 C6 119.6(6) . . ? C7 C8 C8 119.6(4) . 2_675 ? C7 C8 H8A 120.2 . . ? C8 C8 H8A 120.2 2_675 . ? C7 C9 C9 120.0(4) . 2_675 ? C7 C9 H9A 120 . . ? C9 C9 H9A 120 2_675 . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Bi1 Br2 2.7017(17) . ? Bi1 Br1 2.8416(8) 2_665 ? Bi1 Br1 2.8416(8) 3_655 ? Bi1 Br1 2.8416(8) . ? Bi1 Br1 2.8416(8) 4_565 ? Bi2 Br4 2.6918(18) . ? Bi2 Br3 2.8394(9) . ? Bi2 Br3 2.8394(9) 3_655 ? Bi2 Br3 2.8394(9) 2_665 ? Bi2 Br3 2.8394(9) 4_565 ? N1 C1 1.341(8) . ? N1 C5 1.341(9) . ? N1 C6 1.486(7) . ? C1 C2 1.418(13) . ? C1 H1A 0.95 . ? C2 C3 1.369(12) . ? C2 H2A 0.95 . ? C3 C4 1.396(12) . ? C3 H3A 0.95 . ? C4 C5 1.367(14) . ? C4 H4A 0.95 . ? C5 H5A 0.95 . ? C6 C7 1.521(7) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? C7 C9 1.383(9) . ? C7 C8 1.388(9) . ? C8 C8 1.411(15) 2_675 ? C8 H8A 0.95 . ? C9 C9 1.402(15) 2_675 ? C9 H9A 0.95 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag C1 H1A Br1 0.95 3.04 3.912(8) 154.2 4_565 yes C2 H2A Br3 0.95 2.89 3.677(9) 140.9 7_655 yes C4 H4A Br1 0.95 2.86 3.661(8) 142.4 7_655 yes C5 H5A Br3 0.95 3.11 3.966(9) 151.2 4_566 yes C6 H6A Br3 0.99 2.92 3.851(7) 156.8 4_566 yes C6 H6B Br1 0.99 2.95 3.874(8) 155.6 4_565 yes